FACULTY OF APPLIED SCIENCE

AS230 – BACHELOR OF SCIENCE (HONS) MATERIALS

TECHNOLOGY

MST613 – MATERIALS CHARACTERIZATION

EXPERIMENT 2: X-RAY DIFFRACTION (XRD) TECHNIQUE

Prepared by:

NURFAIZLEEN SYAMEERA BINTI PADZIL (2017883078)

Prepared for :

DR MUZAMIR MAHAT

1st OCTOBER 2019

OBJECTIVES

1. To see how the sample is being prepare.

2. To observe the diffraction pattern of any powder or solid.
3. To observe different spectrum of different samples tested.

INTRODUCTION

In this experiment, we used three different samples which is zinc oxide, zinc and H2O.
All the samples were prepared to undergo the X-ray diffraction technique that we already set to 3
minutes each. The function of this technique is to study the crystal structures and the atomic
spacing. X-ray diffraction happened based on constructive interference of monochromatic X-rays
and also the crystalline sample.
When the X-rays generated by a cathode ray tube and direct towards the sample, the X-
rays will be detected, processed and will be counted. When the sample were scanned through a
range of 2θangles, all possible diffraction directions of the lattice should be attained due to the
random orientation of the powdered material. The determination and understanding of all the
unknown solids are important as it will be used in different areas of study examples in material
science, environmental science, biology and engineering.
For calculation, we can use Bragg’s equation where:

The path difference between two waves:

2 x wavelength= 2 d sin(theta)
For constructive interference between these waves, the path difference must be an
integral number of wavelengths:
n x wavelength= 2x
This leads to the Bragg’s equation:
n x wavelength = 2dsin (theta)
MATERIALS AND APPARATUS

Aluminium sample holder, X-ray diffraction machine, three unknown samples, spatula.

PROCEDURE
**Do not open the chamber while the alarm red light is on
**Never touch the detector (may result in signal off).

1. Three samples were obtained from the instructor and then were placed on an aluminium
sample holder. If powder sample were used, we need to use spatula to spread the powder
evenly on the holder.
2. For the Xpert-pro X-ray diffractometer, the instructions need to be read first before start
operated.
3. Optimum settings were setted as below:
Time constant: 3 minutes for each sample
Range: 25-45oC
Chart speed: Low
4. The aluminium sample holder was inserted into the X-ray diffraction machine.
5. Switch on the start knob and chart recorder (slow) simultaneously, the sample was run on
slow chart speed.
6. After completely done 3 minutes for each sample, switch it off and locate all peaks on the
chart. The values of 2theta were recorded and some necessary calculations need to be done.
7. The type of crystal structure were determined based on the pattern of h,k,l.
RESULTS AND DATA

1. H2O

Table 1 Data Table of X-ray Diffraction Peaks

d= n x wavelength/
2theta theta sin(theta)
2sin(theta) Find (h2+k2+l2) =?

(d /a)2

38.551 19.2755 0.3301 2.3345 √2𝑎 = 2.3345

= 1. 6507
47.695 23.8475 0.4043 1.90526 √3𝑎 = 1.90526
= 1. 1000
√4𝑎 = 1.65000
55.600 27.83 0.4669 1.65000
= 0.8250

69.747 34.8735 0.5718 1.34722 √6𝑎 = 1.34722

= 0.5500
√8𝑎 = 1.16673
82.634 41..3170 0.6602 1.16673
= 0.4125
√9𝑎 = 1.10000
88.980 44.449 0.7003 1.10000
= 0.3667

900
800
i
n 700
t 600
e 500
n
400
s
i 300
t 200
y 100
0
10 20 30 40 50 60 70 80 90
2-theta
2. ZnO

Table 1 Data Table of X-ray Diffraction Peaks

d= n x wavelength/
2theta theta sin(theta)
2sin(theta) Find (h2+k2+l2) =?

(d /a)2

31. 772 15.886 0.2737 2.81415 √1𝑎 = 2.81415

= 2.81415
34.420 17.210 0.2959 2.60345 √4𝑎 = 2.60345
= 1.30173
√2𝑎 = 2.47570
36.256 18.128 0.3111 2.47570
= 1.757059

47.541 23.771 0.4031 1.91107 √5𝑎 = 1.91107

= 0.85466
√2𝑎 = 1.62475
56.602 28.301 0.4741 1.62475
= 1.14887
√10𝑎 = 1.47726
62.858 31.429 0.5214 1.47726
= 0.46715

900
800
i
n 700
t 600
e 500
n
400
s
i 300
t 200
y 100
0
10 20 30 40 50 60 70 80 90
2-theta
3. Zn

Table 1 Data Table of X-ray Diffraction Peaks

d= n x wavelength/
2theta theta sin(theta)
2sin(theta) Find (h2+k2+l2) =?

(d /a)2

36.290 18.145 0.3314 2.47350 √4𝑎 = 2.47350

= 1.23675
38.994 19.497 0.3338 2.30796 √1𝑎 = 2.30796
= 2.30796
√2𝑎 = 2.09154
43.221 21.6105 0.3683 2.09154
= 1.47895

54.321 27.1605 0.4565 1.68746 √5𝑎 = 1.68746

= 0.75465
√10𝑎 = 1.34172
70.075 35.0375 0.5741 1.34172
= 0.42429
√2𝑎 = 1.33250
70.632 35.316 0.5781 1.33250
= 0.94222

800

700
I
N 600
T
500
E
N 400
S
300
I
T 200
Y 100

0
10 20 30 40 50 60 70 80 90
2 THETA
*Wavelength = 1.5418 Å (0.15418 nm) for Cu Ka, assuming n =1 and a=0.564n
DISCUSSION

In this experiment, we used three unknown samples which is in powder and thin film form.
After 9 minutes, we observed from the diffractogram that different peaks were formed for different
samples. Each sample shows different result because we need to know that different materials in
periodic table have different arrangement of atoms. So, the peaks, intensity and structure also
should be different. To differentiate the structure of peaks between crystalline and amorphous,
crystalline material always exhibit sharp diffraction peaks while amorphous does not. If we did
the diffraction at low angle, we can observe more of the amorphous phase than its real percentage
in the mixture. So, from all the three samples that we tested, it can be said that all of them (zinc
oxide, zinc, H2O) have crystalline structure due to the sharp, well-defined peaks.

From the results, we get the peaks in a graph xy-axis where x-axis is the 2theta and y-axis
is intensity which recorded as ‘counts’. For the x-axis, we take 2theta instead of theta due to the
Bragg’s equation. For theta, it is the angle between reflected beam and crystallographic plane.
While for 2theta, it is the angle between transmitted x-ray beam and reflected beam. Here, we want
to observe the transmitted and reflected beam and that is why we take 2theta. The peak position at
2theta is depends on some instrumental characteristic such as wavelength. The dhkl values is known
as intrinsic where the Bragg’s law that we used will be applied to convert the 2theta positions to
dhkl.

From calculations from h,k,l, we can determine type of crystal structure that exist. For zinc
oxide, the crystal structure is hexagonal wurtzite and for zinc, it can be said that it is in hexagonal-
closed packed (HCP). While in H2O, the H2O molecule is arrange in layers of hexagonal rings.
Lastly, in this experiment, we can use either in solids or thin film form. For us to use the wet
powders, we need to considerate first. We can use wet powders as long as it will not change
completely to liquid at the end of the experiment. If the wet powders turn to its original form which
is in dry powders, so it can be used to test and error will not happened for this case. Other sources
of errors that may happen during experiment are the instrument misalignment and specimen
displacement. So, these errors need to be avoided and instrument need to be rechecked to make
sure that we can get the accurate and best result.
CONCLUSION

In conclusion, from the experiment, we finally know the three unknown solution that we
tested. Three of them are zinc, zinc oxide and H2O. They also have crystalline structure due to the
sharp and well-defined peak. We can conclude that this experiment success because we achieved
all the objectives that we aim at first of this experiment.

REFERENCES

1. Uncertainty Estimation of Lattice Parameters measured by X-Ray Diffractions (2016).

Retrieved from http://www.imeko.org/publications/wc-2016/PWC-2016-TC8-008u.pdf

2. Elements of X-ray diffraction, by B.D. Cullity and S.R. Stock, 3rd Edition, Pearson
Education International / Prentice Hall, 2001.

3. G.S. Rohrer, Structure and bonding in Crystalline Materials, Cambridge University Press,
2001.